CN101768737B - Storage method of nickel basket used for measuring oxygen content - Google Patents
Storage method of nickel basket used for measuring oxygen content Download PDFInfo
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- CN101768737B CN101768737B CN2008102473822A CN200810247382A CN101768737B CN 101768737 B CN101768737 B CN 101768737B CN 2008102473822 A CN2008102473822 A CN 2008102473822A CN 200810247382 A CN200810247382 A CN 200810247382A CN 101768737 B CN101768737 B CN 101768737B
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- nickel basket
- nickel
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Abstract
The invention belongs to the storage technical field of a material used for measuring the oxygen content in metal, in particular relates to a storage method of a nickel basket used for measuring oxygen content. The method comprises the following steps: using analytically pure phosphoric acid, glacial acetic acid and nitric acid as raw materials to prepare a mixed acid solution, weighting a certain mixed acid solution of which volume ratio to the nickel basket is 1:1-3:1, heating in a water bath or on a asbestos wire gauze for 25-100s, wherein the temperature of the water bath is 60-85 DEG C; washing the nickel basket cleanly with water and absolute alcohol, air-drying with warm wind; and filling inert gas in a reagent plastic bottle and loading in the nickel basket which is treated by mixed acid to store in a sealing environment. The corrosive effect of the nickel basket which is treated by the method of the invention is good, the obtained oxygen content is low and stable, the uniformity of the oxygen content of the treated nickel basket is high and the range is small. The oxygen content of the nickel basket stored by using the storage method of the invention is basically unchanged in several weeks.
Description
Technical field
The invention belongs to the storage technique field of oxygen determination material in the metal, particularly a kind of storage practice of nickel basket used for measuring oxygen content.
Background technology
The testing method of oxygen level is a rare gas element fused instrumental method in the at present general metal.At this moment the poor effect of some metals such as the titanium or titanium alloy oxygen evolution that metal is contained when heating and melting just needs other material of adding that it is melted better and obtains good oxygen evolution effect, and this material is called fusing assistant.The nickel basket is exactly a kind of good fusing assistant.It is made by nickel wire, and two kinds of specifications are generally arranged:
Heavy 1g and
Heavy 1.5g.Its nickel content of starting material nickel wire general requirement of nickel basket is more than 99.6%, because the height of oxygen level can directly influence the last test result in the nickel basket, therefore, oxygen level in the nickel basket that general requirement is handled well is not more than 20 μ g/g, for high pure metal test, often require that oxygen level is not more than 10 μ g/g even 5 μ g/g in the nickel basket.
Because of the existence of the dirt and the oxide compound on top layer, before being used for test, the nickel basket must be handled and could use.The general treatment process of nickel basket be the mixing acid with acetic acid, phosphoric acid and nitric acid add the thermal etching certain hour wash again, air-dry.The general document of aforesaid method can be found, but grasps by the individual entirely for concrete treatment condition.
The nickel basket can directly use after the nitration mixture corrosion, and also can bottling, it is standby to place.For nickel content less than 99.99% nickel basket, directly after the bottling, because of oxidation in its put procedure needs could use after the acid treatment again.Domestic still do not have patent and propose.The mensuration of oxygen is all used the nickel basket in a lot of metals, handles the nickel basket well with the blank value that obtains and extremely important with the suitable way storage.
Summary of the invention
The storage practice that the purpose of this invention is to provide a kind of nickel basket used for measuring oxygen content.
A kind of storage practice of nickel basket used for measuring oxygen content is characterized in that, this method steps is,
(1) preparation mixed acid solution: with analytically pure phosphoric acid, Glacial acetic acid and nitric acid is raw material, phosphoric acid by volume: Glacial acetic acid: nitric acid=90～100: 50～65: 40～50 ratio, measure above-mentioned three kinds of acid solutions respectively, pour in the beaker, stir, after mixing, be transferred in the vial of containing sour usefulness, airtight preservation is standby;
(2) took by weighing mixed acid solution in 1: 1～3: 1 according to mixed acid solution and nickel basket volume ratio, mixed acid solution and nickel basket are put into beaker;
(3) heat on water-bath or the asbestos gauge, bath temperature is 60～85 ℃, and be 25～100s heat-up time;
(4) after heating is finished, take off beaker, in beaker, add water solution is no longer smoldered in order to avoid contaminate environment;
(5) water and dehydrated alcohol are rinsed the nickel basket well, air-drying with warm wind;
(6) with reagent with being full of rare gas element or high-purity N in the Plastic Bottle
2Gas, the nickel basket after the nitration mixture of packing into is handled, sealing is preserved.
Described nickel basket nickel content is 99.8%.
Described rare gas element is high-purity He gas or Ar gas.
Beneficial effect of the present invention is:
Nickel basket corrosive effect after the present invention handles is good, and the gained oxygen level is low and stable, the nickel basket oxygen level homogeneity height after the processing, and the extreme difference value is little.
Oxygen level is constant substantially after the nickel basket of method storage of the present invention is placed several weeks.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1
A kind of storage practice of nickel basket used for measuring oxygen content, used nickel basket nickel content is 99.8%, this method steps is,
(1) preparation mixed acid solution: with analytically pure phosphoric acid, Glacial acetic acid and nitric acid is raw material, phosphoric acid by volume: Glacial acetic acid: the ratio of nitric acid=100: 56: 44, measure phosphatase 24 00mL, Glacial acetic acid 224mL, nitric acid 176mL respectively, pouring the 1000mL large beaker into stirs, after mixing, be transferred in the vial of containing sour usefulness, airtight preservation is standby;
(2) take by weighing acid solution at 2: 1 according to mixed acid solution and nickel basket volume ratio, mixed acid solution and nickel basket are put into beaker;
(3) on the 2kw electric furnace, heating in water bath, bath temperature are 70 ℃, and be 35s heat-up time;
(4) after heating is finished, take off beaker, in beaker, add water solution is no longer smoldered in order to avoid contaminate environment;
(5) air-drying with warm wind rinsed the nickel basket well by water, dehydrated alcohol successively;
(6) with the reagent of 100mL with being full of rare gas element in the Plastic Bottle, the nickel basket after the nitration mixture of packing into is handled, sealing is preserved.
Nickel basket oxygen level after nitration mixture of the present invention is handled is low and steady, for nickel content less than 99.99% nickel basket, because of oxidation in its put procedure needs could use after the acid treatment again.The present invention charges into protective gas in bottle, can make in the bottle nickel basket oxygen level after placing a few weeks longer constant substantially and can directly use.Directly bottling (not charging into protective gas in the bottle); placing for three weeks compares with the storage practice of nickel basket of the present invention; storage practice is as shown in table 1 to the influence of nickel basket (nickel content 99.8%) oxygen level; because of may be oxidized in the put procedure; and oxidation situation difference, cause measurement result than big-difference, measured 7 times; measurement result shows storage practice of the present invention, and nickel basket oxygen levels are constant substantially after three weeks of placement.
Table 1 holding conditions is to the influence of nickel basket (nickel content 99.8%) oxygen level
Claims (3)
1. the storage practice of a nickel basket used for measuring oxygen content is characterized in that, this method steps is,
(1) preparation mixed acid solution: with analytically pure phosphoric acid, Glacial acetic acid and nitric acid is raw material, phosphoric acid by volume: Glacial acetic acid: nitric acid=90～100: 50～65: 40～50 ratio, measure above-mentioned three kinds of acid solutions respectively, pour in the beaker, stir, after mixing, be transferred in the vial of containing sour usefulness, airtight preservation is standby;
(2) took by weighing mixed acid solution in 1: 1～3: 1 according to mixed acid solution and nickel basket volume ratio, mixed acid solution and nickel basket are put into beaker;
(3) heat on water-bath or the asbestos gauge, bath temperature is 60～85 ℃, and be 25～100s heat-up time;
(4) after heating is finished, take off beaker, in beaker, add water solution is no longer smoldered in order to avoid contaminate environment;
(5) air-drying with warm wind rinsed the nickel basket well by water, dehydrated alcohol successively;
(6) with reagent with being full of rare gas element or high-purity N in the Plastic Bottle
2Gas, the nickel basket after the nitration mixture of packing into is handled, sealing is preserved.
2. the storage practice of a kind of nickel basket used for measuring oxygen content according to claim 1 is characterized in that, described nickel basket nickel content is 99.8%.
3. the storage practice of a kind of nickel basket used for measuring oxygen content according to claim 1 is characterized in that, described rare gas element is high-purity He gas or Ar gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102473822A CN101768737B (en) | 2008-12-29 | 2008-12-29 | Storage method of nickel basket used for measuring oxygen content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102473822A CN101768737B (en) | 2008-12-29 | 2008-12-29 | Storage method of nickel basket used for measuring oxygen content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101768737A CN101768737A (en) | 2010-07-07 |
| CN101768737B true CN101768737B (en) | 2011-09-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008102473822A Expired - Fee Related CN101768737B (en) | 2008-12-29 | 2008-12-29 | Storage method of nickel basket used for measuring oxygen content |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1137297A (en) * | 1993-12-15 | 1996-12-04 | 亨凯尔公司 | Phosphate conversion coating and compositions and concentrates therefor with stable internal accelerator |
| CN101086062A (en) * | 2007-07-09 | 2007-12-12 | 陈历泽 | Strong acid metal surface phosphor passivation and anti-rust agent and its production method |
-
2008
- 2008-12-29 CN CN2008102473822A patent/CN101768737B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1137297A (en) * | 1993-12-15 | 1996-12-04 | 亨凯尔公司 | Phosphate conversion coating and compositions and concentrates therefor with stable internal accelerator |
| CN101086062A (en) * | 2007-07-09 | 2007-12-12 | 陈历泽 | Strong acid metal surface phosphor passivation and anti-rust agent and its production method |
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| Publication number | Publication date |
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| CN101768737A (en) | 2010-07-07 |
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Effective date of registration: 20160719 Address after: Yang Yanlu 101407 Beijing city Huairou District Yanqi Economic Development Zone No. 88 Patentee after: National standard (Beijing) inspection & Certification Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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Granted publication date: 20110907 Termination date: 20171229 |
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